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WO2003031828A1 - Microvalve ajustable et procede de reglage et d'actionnement de cette derniere - Google Patents

Microvalve ajustable et procede de reglage et d'actionnement de cette derniere Download PDF

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Publication number
WO2003031828A1
WO2003031828A1 PCT/IB2002/003999 IB0203999W WO03031828A1 WO 2003031828 A1 WO2003031828 A1 WO 2003031828A1 IB 0203999 W IB0203999 W IB 0203999W WO 03031828 A1 WO03031828 A1 WO 03031828A1
Authority
WO
WIPO (PCT)
Prior art keywords
actuating members
micro valve
array
actuating
temperature
Prior art date
Application number
PCT/IB2002/003999
Other languages
English (en)
Inventor
Alec Ginggen
Original Assignee
Medos S.A.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from EP20010123923 external-priority patent/EP1273808B1/fr
Application filed by Medos S.A. filed Critical Medos S.A.
Priority to BRPI0213130-7A priority Critical patent/BR0213130B1/pt
Priority to JP2003534774A priority patent/JP2005504939A/ja
Priority to CA2462968A priority patent/CA2462968C/fr
Priority to AU2002341249A priority patent/AU2002341249B2/en
Publication of WO2003031828A1 publication Critical patent/WO2003031828A1/fr

Links

Classifications

    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16KVALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
    • F16K99/00Subject matter not provided for in other groups of this subclass
    • F16K99/0001Microvalves
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61MDEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
    • A61M27/00Drainage appliance for wounds or the like, i.e. wound drains, implanted drains
    • A61M27/002Implant devices for drainage of body fluids from one part of the body to another
    • A61M27/006Cerebrospinal drainage; Accessories therefor, e.g. valves
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F15FLUID-PRESSURE ACTUATORS; HYDRAULICS OR PNEUMATICS IN GENERAL
    • F15CFLUID-CIRCUIT ELEMENTS PREDOMINANTLY USED FOR COMPUTING OR CONTROL PURPOSES
    • F15C5/00Manufacture of fluid circuit elements; Manufacture of assemblages of such elements integrated circuits
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16KVALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
    • F16K99/00Subject matter not provided for in other groups of this subclass
    • F16K99/0001Microvalves
    • F16K99/0003Constructional types of microvalves; Details of the cutting-off member
    • F16K99/0011Gate valves or sliding valves
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16KVALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
    • F16K99/00Subject matter not provided for in other groups of this subclass
    • F16K99/0001Microvalves
    • F16K99/0034Operating means specially adapted for microvalves
    • F16K99/0036Operating means specially adapted for microvalves operated by temperature variations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61MDEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
    • A61M2205/00General characteristics of the apparatus
    • A61M2205/35Communication
    • A61M2205/3507Communication with implanted devices, e.g. external control
    • A61M2205/3523Communication with implanted devices, e.g. external control using telemetric means
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16KVALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
    • F16K99/00Subject matter not provided for in other groups of this subclass
    • F16K99/0001Microvalves
    • F16K2099/0069Bistable microvalves
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16KVALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
    • F16K99/00Subject matter not provided for in other groups of this subclass
    • F16K2099/0082Microvalves adapted for a particular use
    • F16K2099/0086Medical applications
    • F16K2099/0088Implanted devices
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16KVALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
    • F16K99/00Subject matter not provided for in other groups of this subclass
    • F16K2099/0082Microvalves adapted for a particular use
    • F16K2099/0094Micropumps
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00Fluid handling
    • Y10T137/6416With heating or cooling of the system

Definitions

  • the present invention relates to a method of setting and/or actuating a multi-stable valve used in fluidic or in micro fluidic applications.
  • Another object of the invention is an adjustable multi stable valve for use in medical devices implanted in a human body.
  • the invention relates to a micro valve having at least two stable states at operating temperature.
  • An opening pressure and a resistance to fluid flow correspond to each state of the valve.
  • the valve may be actuated non- invasively, by telemetry for example, thanks to an external device, providing an adjustable opening pressure valve or alternatively a valve assembly with adjustable resistance to flow.
  • the valve object of the present invention has a wide range of applications in different fields (medical, hydraulics, micro-engineering, ).
  • a shunt system that derives the excess of liquid from the brain to the peritonea or to another cavity of the patient.
  • Some existing shunt systems comprise an adjustable valve that allows the surgeon to modify non-invasively the valve opening pressure after implantation.
  • These existing implantable valves for the treatment of hydrocephalic patients have successfully shown that the feature allowing the surgeon to adjust non-invasively the valve opening pressure after implantation is extremely useful. Nevertheless, there are some drawbacks associated with devices of this type that can be summarised as follows:
  • valve object of the present invention overcomes the problems exposed above by providing a micro valve having at least two stable states at operating temperature.
  • the valve according to the invention does not require energy at rest during normal operation and is insensitive to magnetic fields by design. Since the valve setting may be adjusted without mechanical movement of any parts, the valve is less sensitive to blockage due to an accumulation of bio substances.
  • the actuation concept is based on temperature changes above and below body temperature. Energy is only required to change the valve from one state to the other. Valves for the treatment of hydrocephalic patients, as well as valves for all kind of implantable pumps constitute major applications of that concept that may be extended to other fields.
  • a method for setting and actuating an implantable valve having the steps disclosed in claim 1 as well as a micro valve having the characteristics recited in claim 4 obviates the above mentioned drawbacks.
  • Figure 1 is a graph showing the typical temperature hysteresis of shape memory alloy (SMA).
  • Figure 2 is a graph showing the typical stress-strain characteristics of a shape memory alloy in each of its states.
  • Figure 3 is a schematic perspective top view of a first embodiment of a micro valve according to the invention.
  • Figure 4 is a bottom perspective view according to the first embodiment shown at figure 3.
  • Figure 5 is cross sectional view of the first embodiment of the valve shown at figure 3.
  • Figure 6 is a perspective top view of a second embodiment of a micro valve according to the invention.
  • Figure 7 is perspective bottom view of the second embodiment depicted in figure 6.
  • Figure 8 is schematic cross sectional view of the second embodiment depicted in figure 6.
  • Figure 9 is schematic perspective top view of a third embodiment of a micro valve according to the invention.
  • Figure 10 is a perspective bottom view of the third embodiment depicted in figure 9.
  • Figure 11 is a perspective top view of an implantable assembly incorporating a valve according to the invention, the top cover being exploded.
  • Figure 12 is a perspective view of the assembly depicted in figure 11 with the bottom cover exploded.
  • Figure 13 is a bottom perspective view of the assembly shown at figures 11 and 12.
  • Figure 14 is an exploded perspective view of an implantable pump embodying a valve according to the invention.
  • shape memory alloys hereafter called SMA material.
  • SMA material shape memory alloys
  • SMA material is characterised by reversible metallurgical phase transformations that are activated either by temperature change or by induced stress. Below a range of transition temperature, the material is in the martensitic state, whereas above that temperature range, the material is in the austenitic state.
  • the transformation occurs across a range of temperatures which are commonly named A s (start) and A f (finish) for the transformation from martensitic to austenitic state and M s (start) and M f (finish) for the transformation from austenitic to martensitic state as referenced in figure 1.
  • These transformations are reversible so that the material may be treated to assume different shapes in each of the two phases, and can reversibly switch between the two shapes when transformed from one state to the other. More commonly, the material is treated to only return to a shape upon transformation to the austenitic phase a biasing force, acting against the SMA material returns it to its alternate shape upon transformation to the martensitic phase.
  • the elastic modulus of the SMA material depends on its metallurgical state.
  • Figure 2 shows a typical stress-strain graph of a SMA material in both states. It appears clearly that the austenitic state has a higher elastic modulus than the martensitic state.
  • the stress-strain curve is roughly linear and the Young's modulus corresponds to the slope of the curve in the initial loading region. For materials tested at temperatures just above the A f temperature, if the material is further deformed beyond this initial loading region, it will experience a stress-induced martensitic transformation.
  • the point on the stress-strain curve at which the stress-induced martensitic transformation begins can be called the M s 0 .
  • the elastic modulus In the martensitic state, the elastic modulus is lower than in the austenitic state, and the corresponding M s ⁇ (in this case, the stress required to rearrange the pre-existing martensitic phase) is also lower.
  • the invention makes use of the change in mechanical properties (mainly Young's modulus) of an array of actuators in SMA material when a transition between the two metallurgical states occurs.
  • the SMA material is preferably chosen within SMA materials having a working temperature corresponding to body temperature located between M s and A s . In that case, the material is stable in both states at rest. Heating the material above A f will transform it into austenite (higher modulus material). Cooling the material below M f will transform it into martensite (lower modulus material). While the effect is most pronounced with the temperature of use located between M s and A s , the effect can be observed to some extent at a number of temperatures in the broader range between M f and A f .
  • TiNi (Nitinol) is a good choice for the actuating members of a valve according to the invention as it is biocompatible. Further, TiNi can be manufactured such that body temperature is located between M s and A s .
  • Fine tuning the temperature cycle and the mechanical properties may be achieved by playing with the chemical composition and thermomechanical processing of the material.
  • the micro valve object of the invention comprises an array of actuators or actuating members made of a SMA material that interact either directly with the fluid path or with an elastic mean, the tension of which being modified by said array of SMA actuators.
  • the SMA material is selected to have two stable metallurgical states at the temperature of use, e.g., body temperature.
  • the metallurgical state can be changed either by cooling or by heating the SMA actuator.
  • One of the metallurgical states has a higher elastic modulus, whereas the other state has a lower elastic modulus.
  • the heating is obtained by circulating a current through or in the proximity of the SMA material (Joule effect).
  • the cooling is achieved thanks to a Peltier cell or an array of Peltier cells integrated in the base plate of the valve, in the vicinity of the SMA actuators.
  • the fluid path crosses a base plate 2 having an array of orifices 3, closed by the free extremity of a corresponding array of actuating members 1.
  • the base plate 2 is preferably made of a glass type material like Pyrex for example.
  • the geometry of the orifices 3 is identical across the array, which ensures that the resistance to fluid is the same for each single orifice 3.
  • the array of actuating members 1 comprises, in this embodiment, an elongated body from which extend perpendicularly elongated actuating members. Some other configurations are of course possible.
  • the actuating members 1 are made of SMA material, preferably TiNi, and their geometry is chosen so that each fluid path 3 can be considered as closed when the corresponding actuating member 1 is in the austenitic state and open in the martensitic state.
  • a Peltier cell 4 is integrated in the base plate 2, and allows, once energised, the cooling of the array of actuating members 1.
  • Each actuating member 1 may be heated individually by circulating an electrical current through the connectors 5 bounded to each of the actuating members 1.
  • the valve setting is modified in the following manner. First, the temperature of the array of SMA actuating members 1 is decreased to a temperature substantially lower than M s (preferably below M f ) by energising the Peltier cell 4. This transforms all or part of the actuating members 1 to the martensitic state (lower modulus). Then, at least one actuating member is selected within the array and the temperature of all actuating members 1 except the previously selected is increased to a temperature substantially higher than A s (preferably above A f ) This is achieved by circulating an electrical current through the connectors 5 connected to the actuating members 1. Once the higher temperature is reached, all or part of the actuating members 1 are in the austenitic state (higher modulus) except the selected actuating member which remains all or partially in the martensitic state thus determining the opening pressure of the valve.
  • the array of SMA actuators may be first heated to a temperature at which an austenitic transformation occurs and then at least one selected actuating member is cooled down to a temperature at which a martensitic transformation occurs.
  • an array of Peltier cells is provided. Each Peltier cell forming the array being located in the vicinity of an actuating member so as to enable the individual cooling of each actuating member.
  • each actuating member 1 forming the array can be adjusted for providing different opening pressure depending on which actuating member remains in the martensitic state.
  • Figures 6, 7 and 8 depict another embodiment of a valve with an adjustable opening pressure.
  • the base plate 2 has only one orifice 3 through which the fluid may flow.
  • a ball 6 is maintained in the seat of the orifice 3 thanks to an elastic element like a flexible flat spring 7 for example.
  • the spring 7 need not be made of a SMA material.
  • An array of SMA actuating members 1 is arranged perpendicularly to the spring 7 and the free end of each actuating member 1 interacts with the spring 7.
  • the length of the spring allowed to move freely is restricted.
  • the force applied to the ball is determined by the tension of the spring 7 which varies with the metallurgical states of the actuating members 1.
  • a Peltier cell is integrated in the base plate 2 in the vicinity of the SMA array of actuating members 1. Upon activation, the Peltier cell cools the array and all the actuating members 1 change to martensitic state.
  • Each of the actuating members 1 may then be individually heated to a temperature at which an austenitic transformation occurs. This determines the length of activation of the spring 7 and therefore the opening pressure of the valve.
  • a third embodiment of a valve according to the invention provides a valve with an adjustable resistance to flow.
  • a circular base plate 9 comprises, on its periphery, an array of openings 10 through which a fluid may flow.
  • An array of actuating members 11 is arranged on the base plate 9 so that the free end of each actuating member 11 closes a corresponding opening 10 of the base plate.
  • the SMA actuating members 11 are preferably extending from the centre of the base plate 9 to the periphery of said plate.
  • all the actuating members 11 have the same geometry but the geometry of the orifices 10 may differ in order to provide a range of different resistances to flow.
  • a Peltier cell or an array of Peltier cells is integrated in the base plate 9, preferably in the centre of the base plate so as to enable cooling of the complete array of SMA actuating members 11.
  • the setting or the actuating of the valve is similar to what has been disclosed in reference to the first embodiment at figure 3 to 5.
  • FIG. 11 , 12 and 13 illustrate an implantable valve with adjustable opening pressure.
  • the implantable valve comprises a valve assembly 12 according to one of the first or second embodiment disclosed above.
  • a top cover 13 having a fluid outlet 14 is adapted to receive the valve assembly 12.
  • An antenna 17 as well as the necessary electronic components 18 to power and control the valve assembly by telemetry are integrated on the bottom of the base plate of the valve assembly 12.
  • a bottom cover 15 having a fluid inlet 16 and a leak tight compartment 19 for protecting the electronic components closes the structure.
  • the user may then power the assembly by telemetry and select non- invasively the opening pressure from outside the body by firstly cooling the SMA array of actuating members 11 and then selectively heating by Joule effect one or more actuating members 11.
  • the electronic components 18 integrate a feedback mechanism that can be used to confirm that the correct actuating member 11 or array of actuating members have been heated.
  • a valve according to the invention may also be used in an implantable drug delivery pump.
  • a few existing adjustable implantable pumps allow the user (patient and/or doctor) to select non-invasively a flow rate of chemicals to inject, thanks to an external programming unit.
  • the existing devices can be divided in two main categories: the active or passive pumping mechanisms.
  • a battery energises a pump that regulates the flow rate of chemicals.
  • a pressure reservoir "pushes" the chemicals out of the pump.
  • the later concept is very elegant since the pumping does not require energy. Nevertheless, the regulation of the fluid flow is ensured by a valve, the opening of which depends on the power delivered to the valve. Therefore, a battery is still required.
  • valve according to the invention when used in an implantable adjustable pump, the energy consumption problem is solved, since energy is only required to change the flow setting of the pump.
  • the implantable pump comprises a pressurised reservoir 20 that contains the drug substance to administrate.
  • a valve assembly 21 as described with reference to the third embodiment shown in figures 9 and 10 constitutes the adjustable flow resistance valve of the pump.
  • the bottom of the base plate of the valve assembly 21 incorporates electronic components and an antenna that are used to power and control the valve non invasively by telemetry.
  • a leak tight cover 22 protects the bottom face of the base plate and the electronics components, avoiding contact with the pressurised liquid contained in the reservoir 20.
  • a top cover 23 having a fluid outlet 24 closes the structure.
  • the user may select the resistance of the valve from outside with a dedicated reading unit and therefore regulates the outflow of chemicals contained in the pressurised reservoir.
  • valve has multi stable states, energy is only required to switch from one state to the other. No energy is needed to maintain a selected state.
  • Each state can either correspond to a selected opening pressure or to a flow resistance, depending on the application.
  • valve settings can be adjusted without a movement of any part. Only the elastic modulus of the material is modified and therefore the valve is less sensitive to blockage by clogs and other bio-substances.
  • the energy required is the energy needed to power a Peltier cell, and the energy for heating the actuating members. This energy can be provided to the implantable device by telemetry avoiding the use of batteries.
  • the choice of the SMA material is of importance. It must be chosen from the SMA materials that have two stable states at a temperature in the vicinity of the body temperature. Furthermore, the SMA material ideally should fulfill the following conditions. M s ⁇ T ⁇ A s where T is the temperature of the human body and an hysteresis ⁇ T, comprised between 10 and 40 degrees centigrade. TiNi (Nitinol) is a material that fulfills these requirements and which is also biocompatible.

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  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • Biomedical Technology (AREA)
  • Neurology (AREA)
  • Heart & Thoracic Surgery (AREA)
  • Physics & Mathematics (AREA)
  • Theoretical Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Computer Hardware Design (AREA)
  • Ophthalmology & Optometry (AREA)
  • Otolaryngology (AREA)
  • Anesthesiology (AREA)
  • Fluid Mechanics (AREA)
  • Hematology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Temperature-Responsive Valves (AREA)
  • Prostheses (AREA)
  • Micromachines (AREA)
  • Electrically Driven Valve-Operating Means (AREA)

Abstract

La présente invention concerne un procédé de réglage ou d'actionnement d'une microvalve destinée à des applications fluidiques, lequel procédé consiste à refroidir un réseau d'organes d'actionnement réalisés dans un matériau d'alliage à mémoire de forme (SMA) jusqu'à une température inférieure ou égale à la température à laquelle se produit une transformation de l'état austénitique à l'état martensitique de façon que la totalité du réseau d'organes d'actionnement en SMA se trouve entièrement ou partiellement à l'état martensitique, à choisir ensuite au moins l'un des organes d'actionnement correspondant à une pression d'ouverture ou à une résistance à l'écoulement prédéterminée, et à chauffer individuellement chacun des organes d'actionnement, à l'exception de celui qui a été choisi auparavant, jusqu'à une température supérieure ou égale à la température à laquelle se produit une transformation de l'état martensitique à l'état austénitique. L'invention se rapporte également à une microvalve comprenant un réseau d'organes d'actionnement réalisés dans un matériau d'alliage à mémoire de forme.
PCT/IB2002/003999 2001-10-06 2002-09-30 Microvalve ajustable et procede de reglage et d'actionnement de cette derniere WO2003031828A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
BRPI0213130-7A BR0213130B1 (pt) 2001-10-06 2002-09-30 Método para regular uma microválvula ajustável, microválvula ajustável, arranjo de microválvula implantável e bomba implantável
JP2003534774A JP2005504939A (ja) 2001-10-06 2002-09-30 多安定型のマイクロバルブおよび可調整型のマイクロバルブを設定および作動する方法
CA2462968A CA2462968C (fr) 2001-10-06 2002-09-30 Microvalve ajustable et procede de reglage et d'actionnement de cette derniere
AU2002341249A AU2002341249B2 (en) 2001-10-06 2002-09-30 Method of setting and actuating a multi-stable micro valve and adjustable micro valve

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP01123923.3 2001-10-06
EP20010123923 EP1273808B1 (fr) 2001-07-02 2001-10-06 Micro-soupape réglable et procédé de réglage et manoeuvre

Publications (1)

Publication Number Publication Date
WO2003031828A1 true WO2003031828A1 (fr) 2003-04-17

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PCT/IB2002/003999 WO2003031828A1 (fr) 2001-10-06 2002-09-30 Microvalve ajustable et procede de reglage et d'actionnement de cette derniere

Country Status (6)

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US (2) US6926246B2 (fr)
JP (1) JP2005504939A (fr)
AU (1) AU2002341249B2 (fr)
BR (1) BR0213130B1 (fr)
CA (1) CA2462968C (fr)
WO (1) WO2003031828A1 (fr)

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US20030155539A1 (en) 2003-08-21
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US6926246B2 (en) 2005-08-09
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